Beverage manufacture, processing, packaging and dispensing using electrochemically activated water

ABSTRACT

A system using electrochemically-activated water (ECAW) for manufacturing, processing, packaging, and dispensing beverages including: (a) using ECAW to neutralize incompatible residues when transitioning from the production of one beverage to another; (b) using ECAW to rehabilitate and disinfect granular activated charcoal beds used in the feed water purification system; (c) producing a carbonated ECAW product and using the carbonated ECAW for system cleaning or disinfecting; (d) using ECAW solutions in the beverage facility clean-in-place system to achieve improved microbial control while greatly reducing water usage and reducing or eliminating the use of chemical detergents and disinfectants; (e) further reducing biofilm growth in the processing system, and purifying ingredient water without the use of chlorine, by adding an ECAW anolyte to the water ingredient feed stream; and/or (f) washing the beverage product bottles or other packages with one or more ECAW solutions prior to packaging.

This application claims the benefit of U.S. Provisional PatentApplication Ser. No. 61/026,960 filed on Feb. 7, 2008 and incorporatessaid provisional application by reference into this document as if fullyset out at this point.

FIELD OF THE INVENTION

This invention relates to the use of, and to products produced by theuse of, electrochemically activated (ECA) water during the production,processing, packaging (e.g., bottling, canning, etc.), and/or dispensingof water, fruit juice, carbonated soft drinks, sports drinks, fermentedbeverages, brewed beverages, and other beverages.

BACKGROUND OF THE INVENTION Beverage Processing and Packaging

It is well established within beverage production and packagingfacilities that highly sanitary conditions, and effective protocolstherefor, must be maintained in order to satisfy internal qualityassurance requirements and meet batch release specifications.

With progressively more diverse beverage types being developed,manufactured, and packaged within the same facility using the sameproduction lines, the pressure to increase productivity and stillaccommodate the reliable supply of an expanding number of differentproduct varieties necessitates effective cleaning and disinfectingstrategies to prevent microbial contamination and to prevent thecarryover of residual contaminating ingredients (e.g., flavors, colors,alcohol content, etc.) between different batches and product types.

Given that most beverage manufacturing and packaging equipment is partof a permanent installation (i.e., the individual system componentscannot conveniently be removed and separately treated), the cleaning anddisinfection thereof requires the introduction and circulation ofdedicated agents throughout the entire system, rather than allowingspecific individual interventions which would necessitate that theequipment be disassembled and manually cleaned and disinfected.“Cleaning-in-Place” (CIP) thus refers to the practice of circulatingcleaning and disinfecting agents throughout the entire assembly ofsystem components, equipment, and subsystems. “Cleaning-out-Place”(COP), on the other hand, refers to those procedures whereindisassembled equipment and removable fixtures are cleaned anddisinfected separately and largely by hand at stations away from thepermanent manufacturing and packaging systems.

The diverse products that are prepared and packaged within the samefacility using the same filling equipment can often even comprise bothalcoholic and non-alcoholic products. The packaging conditions for allsuch products is governed by the same stringent cleaning anddisinfection prescriptions that are mandated to preclude crosscontamination that would apply between highly flavorful and odor intenseproducts and bottled water. Optimal removal of these robust flavors oralcoholic residues remains a primary limitation to the quick cleaningand turn-around of the filling line and contributes to the large amountof water typically consumed during line and filler head cleaning whenswitching between incompatible and non-benign products.

Aside from the ubiquitous likelihood of microbial contamination and theassociated potential for product spoilage and deterioration, furtherproduct quality criteria that must comply with internal batch releasespecifications include color, taste, smell, and overall character suchas foaming ability and beverage consistency.

Conventional measures heretofore used to address these concerns andlimitations have comprised: the use of solutions or remedies heated tosubstantially elevated temperatures; the use of increased liquid andgaseous pressures; the use of high fluid circulation rates; and extendedexposure to high concentrations of caustic detergents and potentiallyhazardous biocidal compounds.

However, these measures, whilst being largely effective for cleaning andsanitation, remain substantially deficient in terms of (a) the loss ofproductivity resulting from the current inability in the industry toquickly switch the processing line from one product to another and (b)the high energy, potable water, and labor demands of the priorprocedures. In addition to controlling the high cost of other items inthe manufacture and packing process, water consumption also remains apivotal criterion for production efficiency measurement and management.

Besides the cleaning and sanitization procedures discussed above,further measures are typically used to ensure the quality of process andingredient water used in beverage processing plants. Such proceduresinclude a variety of filtration technologies including the use ofsynthetic membranes of varying porosities and the use of GranularActivated Charcoal (GAC) beds or columns for the ‘scrubbing’ ofpartially processed water to achieve selective removal of hazardouspesticides and fungicides, toxins, inorganic compounds, and organicresidues or contaminants.

Unfortunately, any filtration technology, whether membrane based and/orGAC in type, will continuously trap the agents or elements that arebeing filtered. These filtrates progressively accumulate to the pointthat the selective separation efficiency of the system is compromised.The maintenance and rejuvenation of these fouled filtration systems hasthus heretofore required either (a) costly and largelynon-environmentally friendly intermittent replacement of the corefiltration components or (b) physical (heat) and/or chemicalinterventions to rehabilitate and restore the systems to functionalefficiency

The discharge of large volumes of soiled effluent solutions (e.g.,effluents containing beverage ingredients, disinfectants, cleaningchemicals, etc.) into waste water reticulation systems is also animportant environmental constraint to optimal beverage production andpackaging capacity. Steps to limit the amounts of CIP chemicals and/orbeverage contaminants in the effluent streams include the installationof systems to recover and store the different chemical agents forre-use, as well as efforts to limit the amount of rinse water used toremove the chemical residues from the diverse systems after cleaning anddisinfection. While more efficient and judicious water and chemicalusage provides a degree of improvement in the quantity and quality ofthe effluent discharge, the quality and quantity of the effluentdischarge continues to constitute a critical production constraint inbeverage manufacturing and packaging facilities.

Aside from the need to enhance the degree of efficiency and qualitycompliance achieved during the manufacture and packaging of beverageproducts, it is also critical to the maintenance of final productintegrity that due effort be invested in ensuring that beveragedispensing systems (e.g., water and soda fountains and draft beerdispensers) be similarly cleaned of residual product and disinfected.Product residues serve as a medium for further microbial growth and,thus, biofilm development, and have an adverse impact upon dispensedproduct quality, health, and safety.

Consequently, in a production environment where there is a great deal ofpressure to optimize the productivity of existing fixed assets (i.e.,processing and packaging lines, etc.) and where there is a progressivelyheightened consumer and shareholder awareness and disapproval of theinefficient usage of resources, a great need exists for a more holisticand progressively renewable approach to cleaning and sanitation in orderto realize sustainable quality assurance and enhanced productivity.

Electrochemically Activated Water (ECA)

It is well known that electrochemically activated (ECA) water can beproduced from diluted dissociative salt solutions by passing anelectrical current through the electrolyte solution in order to produceseparable catholyte and anolyte products. The catholyte, which is thesolution exiting the cathodal chamber, is an anti-oxidant whichtypically has a pH in the range of from about 8 to about 13 and anoxidation-reduction (redox) potential (ORP) in the range of from about−200 mV to about −1100 mV. The anolyte, which is the solution exitingthe anodal chamber, is an oxidant which typically has a pH in the rangeof 2 to about 8, an ORP in the range of +300 mV to about +1200 mV and aFree Available Oxidant (FAO) concentration of ≦300 ppm.

During electrochemical activation of aqueous electrolyte solutions,various oxidative and reductive species can be present in solution, forexample: HOCl (hypochlorous acid); ClO₂ (chlorine dioxide); OCl⁻(hypochlorite); Cl₂ (chlorine); O₂ (oxygen); H₂O₂ (hydrogen peroxide);OH⁻ (hydroxyl); and H₂ (hydrogen). The presence or absence of anyparticular reactive species in solution is predominantly influenced bythe derivative salt used and the final solution pH. So, for example, atpH 3 or below, HOCl tends to convert to Cl₂, which increases toxicitylevels. At a pH below 5, low chloride concentrations tend to produceHOCl, but high chloride concentrations typically produce Cl₂ gas. At apH above 7.5, hypochlorite ions (OCl⁻) are typically the dominantspecies. At a pH>9, the oxidants (chlorites, hypochlorites) tend toconvert to non-oxidants (chloride, chlorates and perchlorates) andactive chlorine (i.e. defined as Cl₂, HOCl and ClO⁻) is typically lostdue to conversion to chlorate (ClO₃ ⁻). At a pH of 4.5-7.5, thepredominant species are typically HOCl (hypochlorous acid), O₃ (ozone),O₂ ²⁻ (peroxide ions) and O₂— (superoxide ions).

For this reason, anolyte will typically predominantly comprise speciessuch as ClO; ClO⁻; HOCl; OH⁻; HO₂; H₂O₂; O₃; S₂O₈ ²⁻ and Cl₂O₆ ²⁻, whilecatholyte will typically predominantly comprise species such as NaOH;KOH; Ca(OH)₂; Mg (OH)₂; HO⁻; H₃O₂ ⁻; HO₂ ⁻; H₂O₂ ⁻; O₂ ⁻; OH⁻ and O₂ ²⁻.The order of oxidizing power of these species is: HOCl(strongest)>Cl₂>OCl⁻ (least powerful). For this reason, anolyte has amuch higher antimicrobial and disinfectant efficacy in comparison tothat of catholyte, or of commercially available stabilized chlorineformulations used at the recommended dosages.

SUMMARY OF THE INVENTION

The present invention satisfies the needs and alleviates the problemsdiscussed above. The benefits of the invention include, but are notlimited to: microbial decontamination; reducing or eliminating the needfor harmful cleaning and disinfection chemicals; biocide potentiation;elimination of pesticide contaminants; and odor and flavor residueneutralization, in the processed, packaged and/or dispensed product, theprocessing infrastructure, and the packaging containers.

In one aspect, there is provided a method of transitioning at least aportion of a beverage processing system from processing a first beverageto processing a second beverage wherein the first beverage includes amaterial which is not compatible with the second beverage and an amountof material remains in the beverage processing system after processingthe first beverage. The material can be a substance which imparts aflavor, a substance which imparts a color, an alcohol, a substance whichimparts a smell, or a combination thereof. The method comprises thesteps of: (a) delivering an amount of an electrochemically-activatedwater anolyte solution through the portion of the beverage processingsystem effective for oxidizing at least a portion of the materialtherein and then (b) processing the second beverage in the portion ofthe beverage processing system. The portion of the material oxidized bythe electrochemically-activated water anolyte solution in step (a) is anamount sufficient such that the material will not prevent the secondbeverage from meeting a release requirement for taste, smell, color,alcohol content, or a combination thereof. Theelectrochemically-activated water anolyte solution can be used in step(a) in undiluted form or can be delivered through the portion of thebeverage processing system in step (a) as an aqueous dilution of theelectrochemically-activated water anolyte solution.

As used herein and in the claims, the term “beverage processing system”refers to the entire production and packaging system for any givenbeverage. The entire system can comprise an assembly of numerousdifferent portions including all lines and subsystems for producing andpackaging the product. Examples of such lines and subsystems include,but are not limited to, ingredient delivery systems, ingredient mixingsystems, fill lines for filling bottles or other packages andintermediate processing systems for heating, cooling, or carbonation,and/or subsystems for conducting other production procedures.

In another aspect, there is provided a method comprising the use of anon-toxic ECAW (preferably the catholyte or an aqueous catholytedilution) as a cleaning agent for the removal of residual beverage soilsfrom beverage production and packaging equipment. This cleaning agentmay be included in the clean-in-place (CIP) procedure at ambienttemperatures and, relative to conventional alkaline caustic soda basedcleaning formulations, the ECAW is substantially free-rinsing, thusobviating the need for a mandatory large-volume, post-caustic waterrinse. Thus, in a further aspect of the invention, the inventive methodenhances water efficiency. Also in this regard, the intrinsiccompatibility of the catholyte solution used for cleaning with theoxidant anolyte solution used for terminal disinfection permits thesequential and tandem application of the two solutions (catholyte andthen anolyte) without the need for an intermediate rinse step. Thedisinfecting properties of the anolyte solution are not compromised byresidual catholyte carry-over.

In another aspect, there is provided a method comprising the use ofelectrochemically activated water (ECAW) (preferably anolyte or anaqueous anolyte dilution) as a non-toxic disinfecting remedy in theproduction and packaging of diverse beverages types. The ECAW preferablyincludes HOCl, which is more effective at killing harmful pathogens thanhypochlorite. This remedy also has the advantage of being substantiallyeffective at ambient temperatures and obviates the need for hightemperature manipulations of the disinfectant wash solutions to achieveequivalent levels of microbial control.

In another aspect, there is provided an improved process forcleaning-in-place at least a portion of a beverage processing systemwherein the process uses an overall total volume of water and theprocess has comprised the steps of (a) delivering an amount of anaqueous rinse through the portion of the beverage processing system andthen (b) delivering an amount of an aqueous disinfectant solutionthrough the portion of the beverage processing system, the amount of theaqueous rinse and the amount of the aqueous disinfectant solutiontogether being effective to attain a level of microbial control therein.The improvement comprises reducing the overall total volume of waterused in the process and reducing the amount of the aqueous disinfectantsolution used in step (b) while still obtaining at least the same levelof microbial control. This is achieved by using anelectrochemically-activated water anolyte solution as the aqueousdisinfectant solution in step (b).

In another aspect of the inventive clean-in-place process, the inventiveimprovement preferably also comprises further reducing the overall totalvolume of water used in the process and reducing the amount of theaqueous rinse used in step (a) while still obtaining at least the samelevel of microbial control. This is achieved by using an aqueouselectrochemically-activated water anolyte dilution as the aqueous rinsein step (a).

Examples of beverage processing systems wherein the improvedclean-in-place process can be used include, but are not limited to,systems for processing carbonated soft drinks, brewed beverages, fruitbeverages, fermented beverages, vegetable beverages, sport drinks,coffee beverages, tea beverages, or combinations thereof. As anotherexample, the improved clean-in-place process can also be used inbeverage processing systems for providing bottled or packaged water.

In another aspect, there is provided an improved process forcleaning-in-place at least a portion of a beverage processing systemwherein the process uses an overall total volume of water and theprocess has comprised the steps of (a) delivering an amount of anaqueous cleaning solution through the portion of the beverage processingsystem, then (b) delivering an amount of an intermediate aqueous rinsethrough the portion of the beverage processing system, and then (c)delivering an amount of an aqueous disinfecting solution through theportion of the beverage processing system, wherein the amount of theaqueous cleaning solution, the amount of the intermediate aqueous rinse,and the amount of the aqueous disinfecting solution together have beeneffective to obtain a level of microbial control in the portion of thebeverage processing system. The improvement comprises reducing theoverall total volume of water used in the process and reducing theamount of the aqueous cleaning solution used in step (a) and the amountof aqueous disinfecting solution used in step (c) while still obtainingat least the same level of microbial control. This is achieved by: (i)using an electrochemically-activated water catholyte solution as theaqueous cleaning solution in step (a); (ii) using anelectrochemically-activated water anolyte solution as the aqueousdisinfecting solution in step (c); and (iii) reducing the amount of oreliminating the intermediate aqueous rinse in step (b).

In another aspect, there is provided a method of rehabilitating anddisinfecting a Granular Activated Charcoal (GAC) bed used for purifyingwater. The method comprises the non-simultaneous steps of: (a)contacting the GAC bed with an electrochemically-activated watercatholyte solution and (b) contacting the GAC bed with anelectrochemically-activated water anolyte solution.

In the method of rehabilitating and disinfecting a GAC bed, theelectrochemically-activated water anolyte solution will have a beginningoxidation-reduction potential prior to contacting the GAC bed and willhave a spent oxidation-reduction potential after being used forcontacting the bed. The beginning oxidation-reduction potential of theelectrochemically-activated water anolyte solution will preferably be apositive mV oxidizing value. In addition, step (b) of the methodpreferably comprises the steps of: (i) determining the beginningoxidation-reduction potential of the electrochemically-activated wateranolyte solution, (ii) contacting the GAC bed with theelectrochemically-activated water anolyte solution, (iii) determiningthe spent oxidation-reduction potential of theelectrochemically-activated water anolyte solution after step (ii), and(iv) repeating steps (ii) and (iii) at least until the spentoxidation-reduction potential of the electrochemically-activated wateranolyte solution determined in step (iii) is a positive mV oxidizingvalue which is not more than 544 mV less than the beginningoxidation-reduction potential prior to step (ii). More preferably, instep (iv), steps (ii) and (iii) will be repeated at least until thespent oxidation-reduction potential of the electrochemically-activatedwater anolyte solution is not more than 143 mV, most preferably not morethan 104 mV, less than the beginning oxidation-reduction potential.

In addition, step (ii) of the method for rehabilitating and disinfectinga GAC bed is preferably conducted at least twice such that: (1) theelectrochemically-activated water anolyte solution is at least oncedelivered to the GAC bed in a substantially normal operating flowdirection and (2) the electrochemically-activated water anolyte solutionis at least once delivered to the GAC bed in a reverse flow directionwhich is substantially opposite the substantially normal operating flowdirection. Similarly, step (a) of the method for rehabilitating anddisinfecting a GAC bed is also preferably conducted at least twice suchthat (1) the electrochemically-activated water catholyte solution is atleast once delivered to the GAC bed in a substantially normal operatingflow direction and (2) the electrochemically-activated water catholytesolution is at least once delivered to the GAC bed in a reverse flowdirection which is substantially opposite the substantially normaloperating flow direction.

In another aspect, there is provided a method of treating GranularActivated Charcoal (GAC) columns used in beverage production, or innon-beverage systems, for the filtration of process water and theadsorption of noxious impurities and chemical contaminants. In theinventive method, the rehabilitation and regeneration of the carbongranules is preferably achieved by the strategic tandem introduction ofECA solutions as a substitute, or at least as a supplement, forconventional thermal or chemical regeneration procedures.

In another aspect, there is provided a method of disinfecting GranularActivated Charcoal (GAC) filtration systems wherein the contaminatedadsorption surfaces within the pores of the carbon granules are exposedto an ECAW oxidant solution (preferably anolyte or an aqueous anolytedilution) which facilitates both (a) the removal of microbial coloniesand established biofilm, and (b) the elimination of both sessile andplanktonic microbe species within the GAC system. The inventive methodreduces or eliminates the need for noxious chemical, high temperature,and pressurized steam interventions of the type heretofore used forsanitizing such systems.

In another aspect, there is provided a method of predicting the biocidalperformance of the ECA solutions whilst circulating in a GAC system bymeasuring the physio-chemical attributes of both the influent andeffluent streams of the ECA treatment solution. By this method, the rateof ECA solution replenishment relative to the residual surface chargewill afford a relative correlate to the measure of Oxidant ReductionPotential (ORP), and hence the volume of each specific ECA solution thatwill need to be applied to the GAC system in order to effect optimalbiofilm removal and microbial elimination and to regenerate adsorptioncapacity of the GAC system.

In another aspect, there is provided a method comprising the in-processintroduction of food-grade, aqueous-based ECAW biocide for use duringthe manufacture and packaging of beverage products, the method beingparticularly effective for the terminal control of superficial microbialbiofilm growth, this with a resultant reduction of recontamination ofpackaged product from the same biofilm associated spoilage andpathogenic microbes.

In another aspect, there is provided a method of at least reducingbiofilm growth in a beverage processing system having a water ingredientfeed stream. The method comprises the step of adding anelectrochemically-activated water anolyte solution to the water feedstream in an amount not exceeding 20 parts by volume of theelectrochemically-activated water anolyte solution per 80 parts byvolume of the water ingredient feed stream.

In another aspect, there is provided an improved process for producing abeverage product wherein the process includes placing the beverageproduct in product packages. The improvement comprises the step, priorto placing the beverage product in the packages, of washing the productpackages using an electrochemically-activated water catholyte solution.The product packages treated in accordance with this process can bebottles or other types of containers. The improvement also preferablycomprises the step, prior to the step of washing, of spraying, soaking,or otherwise contacting the product packages in anelectrochemically-activated water anolyte solution.

In another aspect, there is provided a method of potentiating anelectrochemical property (e.g., pH, oxidation-reduction potential, freeactive oxidant content, and/or electrical conductivity) of anelectrochemically-activated water solution comprising the step ofdissolving CO₂ in the electrochemically-activated water solution toproduce a carbonated product solution. The electrochemically-activatedwater solution can be an anolyte solution, a catholyte solution, or acombination thereof and can be in undiluted or in aqueous dilution form.

In another aspect, there is provided a carbonated composition comprisingan electrochemically-activated water solution having an effective amountof CO₂ dissolved therein to produce a positive mV change in anoxidation-reduction potential of the electrochemically-activated watersolution. The electrochemically-activated water solution can be ananolyte solution, a catholyte solution, or a combination thereof and canbe either in undiluted form or in the form of an aqueous dilution.

In another aspect, there is provided a method cleaning or disinfectingat least a portion of a food processing system comprising the step oftreating the portion of the food processing system with a carbonatedsolution comprising an electrochemically-activated water solution havingan effective amount of CO₂ dissolved therein to produce a positive mVchange in an oxidation-reduction potential of theelectrochemically-activated water solution. Theelectrochemically-activated water solution can be an anolyte solution, acatholyte solution, or a combination thereof and can be in undiluted orin aqueous dilution form.

In another aspect, there is provided a method to potentiate the biocidalactivity of an oxidant ECA solution comprising the introduction ofgaseous carbon dioxide (CO₂) into the ECAW or diluted ECAW to carbonateor pressurize the ECA solution. Thus, there is also provided a methodcomprising the introduction of carbonated ECAW, or a carbonated aqueousdilution of ECAW, into the production, processing and packaging systemand infrastructure and/or elsewhere in the beverage production andpackaging system, or into a non-beverage system. Using REDOX potential(ORP) as a reliable predictor of biocidal activity, it has beendiscovered in accordance with the present invention that, with the useof a carbonated ECA solution, a reduced amount and/or rate of ECAW isneeded, when contrasted with non-carbonated oxidant ECA solutions, toachieve a given level of antimicrobial efficacy.

The specific introduction of CO₂ during the disinfection of the beveragemixing and filling equipment additionally serves to assure optimaldisinfection by increasing the exposure of the “CO₂ potentiated oxidant”to all aspects of the filling and mixing equipment. Conventionalpressure gradients driven by supply pumps within the beverage fillerequipment may not afford adequate disinfectant distribution efficiencyfor optimal antimicrobial effect.

The surprising and unexpected increase in potency of aqueous diluteanolyte solutions which have been “carbonated” with CO₂ allows theamount of anolyte used in any particular application to be reducedwithout compromising antimicrobial activity. One benefit of thisdiscovery is the further minimization of any potential adverse impactthat the anolyte might have when used in conjunction with high risk,ultra sensitive products such as bottled water andpreservative-formulations such as iced coffee wherein taste, color, andconsistency are critical elements of the product's constitution.

The carbonation of water-based beverages with CO₂ gas typically resultsin the formation of an amount of carbonic acid (H₂CO₃). It is believedthat the increased disinfecting potency of the inventive carbonatedanolyte may, to some extent, result from the formation of an amount ofcarbonic acid in the carbonated aqueous anolyte solution.

In yet another aspect, there is provided a method comprising treatingbeverage production and packaging equipment with ECAW or aqueous dilutedECAW at ambient temperatures to neutralize the residual odor and tasteof flavorant ingredients that conventionally require both protractedexposure to high temperature caustic detergent solutions and extendedwater rinse cycles.

In another aspect, there is provided an ECAW solution, and a methodcomprising the application of the ECAW solution, for the improvedremoval and elimination of alcohol-containing residues from beverageproduction systems, containers, and packaging system infrastructure.

In another aspect, there is provided a method of using ECAW as acleaning agent, a sanitizing agent, and/or an ingredient in theproduction, processing, and packaging of beverages of all types. Themethod eliminates chemical pesticide, fungicide and herbicide residueswhich may be harmful to the integrity of the beverage and the health ofthe consumer. Such residues are common contaminants in process watersupplies deriving, for example, from areas of high agricultural activityand pose a significant health and safety risk.

In another aspect, there is provided a method, and an ECAW solutiontherefor, wherein the ECAW solution enhances the antimicrobialbiosecurity of intermediate and pre-packaged products which may besubjected to unplanned transient or extended in-process storage whereunchecked microbial growth would adversely impact upon final productquality.

In another aspect, there is provided a method wherein ECAW is used forthe safe and effective cleaning and decontamination of beveragedispensing systems including, but not limited to, water and sodafountains and draft beer dispensing systems.

Further objects, features, and advantages of the present invention willbe apparent to those of ordinary skill in the art upon examining theaccompanying drawings and upon reading the following detaileddescription of the preferred embodiments.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a chart showing microbial count results obtained in Example 1for packaged product.

FIG. 2 is a chart showing microbial count results obtained in Example 1in filling equipment and containers.

FIG. 3 is a chart showing microbial count results obtained in Example 1for the final rinse wash.

FIG. 4 is a flow diagram illustrating an embodiment 2 of an improvedsoft drink production, processing, and packaging system provided by thepresent invention.

FIG. 5 is a flow diagram illustrating an embodiment 6 of an improvedbottled water production system provided by the present invention.

FIG. 6 is a flow diagram illustrating an embodiment 10 of an improvedfruit juice production and packaging system provided by the presentinvention.

FIG. 7 is a flow diagram illustrating an embodiment 14 of an improvedwine production and bottling system provided by the present invention.

FIG. 8 is a flow diagram illustrating am embodiment 18 of an improvedbeer production and packaging system provided by the present invention.

FIG. 9 schematically illustrates a method provided by the presentinvention for treating granular activated carbon (GAC) filtrationsystems.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

According to the invention, there is provided an in-process, real-timemethod of biocide intervention wherein ECAW (i.e., anolyte, catholyte,or a combination thereof) is used as a disinfectant and/or detergentduring the production, packaging and/or dispensing of a diverse range ofbeverage products. The inventive method is capable of producingintermediate products and packaged final products which consistentlymeet stringent sanitary specifications.

In one aspect, the inventive method preferably comprises the step ofsanitizing the beverage production and/or packaging systems forintermediate and packaged products (including either (a) substantiallythe entire production line/system, (b) any desired portion thereof, or(c) any selected subsystems) by delivering through the system(s) anelectrochemically activated aqueous anolyte, or an aqueous dilutionthereof. The anolyte used preferably has a pH (undiluted) in the rangeof from about 4.5 to about 7.5, an ORP (undiluted) in the range of fromabout +650 mV to ≧+900 mV, and a free available oxidant (FAO)concentration (undiluted) of ≦300 ppm. The pH (undiluted) of the anolytewill more preferably be in the range of from about 5.5 to about 7.

The anolyte, when added to or delivered through the various phases ofthe process (filtration, sanitization, and ingredient water), will haveand will impart distinctive physiochemical attributes such as pH,electrical conductivity, ORP and Free Available Oxidant (FAO)concentration. These parameters, in turn, have a direct causalrelationship with antimicrobial efficacy based upon an inverserelationship between microbial bioload and anolyte dilution applied. Inother words, higher microbial counts require either (a) a higher anolyteconcentration (i.e., lower dilution) for a shorter exposure time or (b)a longer exposure period for a lower anolyte concentration (i.e.,greater dilution). This reflects the fact that there is a directcorrelation between the measure of the aqueous dilution of the anolyteand the predictable changes in the Electrical Conductivity and FreeAvailable Oxidant concentration being measured in the diluted sample.The pH and ORP changes within the dilution series do not followidentical linear reduction trends. The ORP values tend to remainsubstantially elevated until highly:diluted (1:50-1:100), at which pointthe ORP falls dramatically. pH, on the other hand, tends to remainconstant and to assume the pH value of the diluent water.

These parameters can be measured on a real-time basis so as to reliablypredict the antimicrobial capacity of the anolyte solution at any givenpoint. There is a direct correlation between ORP and predictableantimicrobial activity. High ORP (i.e. ≧600 mV) will yield effectivemicrobial elimination within 5 minutes. This efficacy falls, however,when the ORP is reduced. At low ORP anolyte concentrations and/or highmicrobe levels, antimicrobial activity can be increased as needed byincreasing the exposure time.

The anolyte will preferably be produced by electrochemically activatinga dilute aqueous saline solution comprising in the range of from about 1to about 9 grams of salt per liter of water. The saline solution willpreferably comprise from about 2 to about 3 grams of salt per liter ofwater.

The salt can be any inorganic salt. The salt will preferably benon-iodated sodium chloride (NaCl) or potassium chloride (KCL).

The inventive method can include the step of generating the anolytesolution on site. Various types of equipment and procedures which can beused to produce anolyte having the characteristics described above areknown in the art. As will be understood by those in the art, a preferredprocedure comprises the steps of: electrochemically activating a diluteelectrolyte (salt) solution in an electrochemical reactor comprisinganodal and cathodal chambers from which separable electrochemicallyactivated aqueous anolyte and catholyte solutions (i.e., the“concentrated solutions”) can be produced; separately harvesting thecatholyte solution; reintroducing at least some of the catholytesolution into the anodal chamber in the absence of any fresh water; andmanipulating the flow rate, hydraulic flow configuration and regimen,pressure and temperature of the catholyte through the anodal chamber asneeded so as to produce an anolyte solution that is characterized inthat it predominantly includes the species HOCl (hypochlorous acid), O₃(ozone), O₂ ²⁻ (peroxide ions) and O²⁻ (superoxide ions), and has a FreeAvailable Oxidant (FAO) concentration of ≦300 ppm.

When used in the inventive method as a sanitizing wash for beverageproduction, processing, and packaging systems, the anolyte willpreferably be diluted with water. The diluted anolyte solution willpreferably comprise at least 50 parts by volume of water per 50 parts byvolume of concentrated anolyte. More preferably, the diluted anolytewill have a water-to-anolyte volume ratio of at least 60:40 when used insystems for producing and packaging manufactured beverages such ascarbonated soft drinks and brewed beverages, and will have awater-to-anolyte ratio of at least 50:50 in systems for producing andpackaging fruit based or fermented fruit or vegetable based products. Ineach case, the parts by volume ratio of water to concentrated anolytewill preferably not be greater than 98:2, will more preferably not begreater than 95:5, will more preferably be in the range of from about94:6 to about 60:40, and will most preferably be in the range of fromabout 93:7 to about 65:35.

The anolyte sanitizing wash can desirably be introduced at a temperatureas per standard operating conditions. The anolyte sanitizing wash willpreferably be introduced at a temperature in the range of from about 5°C. to about 45° C.

The inventive method can comprise continuous and/or episodic treatmentinterventions by introduction of the anolyte solution at single and/ormultiple sanitation points or sections of the beverage system so as tomaintain the Oxidation-Reduction Potential (ORP) of the anolyte solutionat desired levels throughout the system being treated, this to furtherensure that the predictive relationship between the minimummicrobiocidal and measured oxidant reactivity of the anolyte sanitizingwash is maintained throughout the system during sanitation.

The inventive method can also include a further step of selectivelyadministering an anti-oxidant, electrochemically activated aqueouscatholyte solution into the beverage production, processing, and/orpackaging system as a free rinsing detergent or surface active agent.The period of exposure required is well within the time constraints ofhigh volume processing and packaging. The catholyte (undiluted) willpreferably have a pH in the range of from about 8 to about 13 and anegative ORP of at least −700 mV.

The inventive method can further include the step of washing any desiredaspect of the beverage system with an anolyte having a pH (undiluted) inthe range of from about 2 to about 5 and an ORP (undiluted) of ≧1000 mV.This distinctive anolyte solution can be applied at any appropriatetreatment point in the beverage system. Examples of particularlybeneficial treatment points include, but are not limited to, bulkholding vessels, fermentation vats, bright beer or synthetic syruptanks, transfer vessels, and/or allied reticulation systems which maycomprise, for example, filtration, separation, dilution, pasteurizationand carbonation systems.

The inventive method can also include the further step of selectivelyapplying anolyte, preferably having a pH (undiluted) in the range offrom about 6.0 to about 6.5, an ORP (undiluted) of ≧+950 mV and a FreeAvailable Oxidant concentration (undiluted) of ≦300 ppm, so as tocontinuously neutralize residual microbial contaminants, as well as toeffect a residual disinfection of downstream process equipment forcontrol of potentially recontaminating biofilm growth. The anolyte willpreferably be introduced into the general process water at aconcentration of up to 20 parts by volume anolyte per 80 parts by volumewater. This step preferably involves low dose inclusion of anolyte, on acontinuous basis, into the general process water stream so as toeliminate newly introduced microbes from the water supply system(municipal authority, borehole, etc.) and to also manipulate the chargeof the treated water to prevent the further or new growth of biofilmwhich might otherwise result from irregular interventions of anolytetreatment during the CIP process or elsewhere. The continuous low doseanolyte application serves to both eliminate new microbes introducedinto the system and to prevent the new growth of biofilm which wouldcreate a new source of microbial contamination over time. The points ofapplication in the overall process flow will preferably correspond withthe targeted microbe to biocide contact period as described by theminimum dwell time within the process, itself correlated with themagnitude of anolyte dilution and the minimum levels of microbialdecontamination required within the treated process water. Typicallylarge batch production volumes will require extended processing time andthus protracted storage and packaging periods.

In accordance with the present invention, examples of points or systemsin typical beverage production processing and packaging units wherecatholyte, either in concentrated or preferably in aqueous diluted form,can be introduced as a cleaning solution include, but are not limitedto: (a) water treatment areas for, e.g., mixing with flocculation andfloor washing; (b) ultra filtration module areas for, e.g., membranecleaning, downstream and upstream disinfection and sterilizing, and as areplacement for detergents and other agents in the Clean-in-Place (CIP)system; (c) soil removal; and (d) chain lube biofilm removal for productdecontamination.

When used for cleaning the interiors of fermentation vessels inbreweries, the catholyte cleaning solution will preferably comprise (a)an electrochemically-activated water catholyte solution and (b) anamount of a food grade non-ionic surfactant effective to reduce, andmost preferably to prevent, foam formation in the fermentation vessel.Without the surfactant, oily organic residues in the fermentation vesselwill cause the formation of a foam which will greatly inhibit thephysical shearing action of the catholyte solution, thus significantlyreducing its cleaning effectiveness. However, I have discovered that theaddition of a relatively small amount of non-ionic surfactant to thecleaning composition is effective for reducing or preventing foamformation, thereby greatly enhancing the cleaning effectiveness of thecatholyte solution.

The electrochemically-activated water catholyte solution used in thefermentation vessel cleaning composition can be in undiluted or inaqueous dilution form and will preferably comprise a catholyte productwhich, when in undiluted form, has a negative oxidation-reductionpotential of at least −110 mV and a pH in the range of from about 8 toabout 13. The catholyte solution will preferably be an aqueous dilutionof the catholyte product comprising at least 50% by volume (morepreferably at least 70% and most preferably at least 80% by volume) ofnonelectrolyzed water based on the total combined volume of thenonelectrolyzed dilution water and the catholyte product.

Examples of non-ionic surfactants suitable for use in the fermentationvessel cleaning composition include, but are not limited to, Biosil AF720F, which is an aqueous emulsion comprising polysiloxane, treatedsilica, and an emulsifier, and polyoxyethylene surfactants. Thenon-ionic surfactant will preferably be used in an amount of at least 10mg per liter of the catholyte cleaning composition (or 10 ppm). Higheramounts of the surfactant will typically be preferred as theconcentration of the catholyte solution increases.

Examples of areas in a typical beverage production processing andpackaging plant where anolyte, either in concentrated or preferably inaqueous diluted form, can be used as a disinfecting wash or agentinclude, but are not limited: (a) water treatment applicationsincluding, e.g., replacing chlorine disinfectants and biofilm removal;(b) ultra filtration module area applications including, e.g., membranecleaning, downstream and upstream disinfection and sterilization, and asa replacement for CIP chemical agents and washes heretofore used in theart; (c) biofilm removal, biofilm control and sugar removal; (d) productdecontamination applications including, e.g., chain lube biofilmremoval, replacement of CIP chemicals heretofore used in the art, andnozzle cleaning; and (e) bottle washing applications including bottleand cap cleaning.

FIG. 4 schematically illustrates a soft drink production processing andpackaging system 2 which has been improved to utilize ECAW at variouspoints and in various subsystems. The soft drink line 2 includes anelectrochemical activation system/reactor unit 4 for producing ananolyte and a catholyte product. Examples of systems, subsystems andpoints wherein concentrated or aqueous diluted catholyte washingsolutions are introduced and used in the soft drink production line 2include: bottle washing; bottle washing caustic bath applications; andin the Clean-in-Place (CIP) system for substantially the entire the line2 or any portion thereof. Examples of systems, subsystems and pointswherein concentrated or aqueous diluted anolyte disinfecting washsolutions are introduced and used in accordance with the presentinvention include: the CIP system for substantially the entire line 2 orany portion thereof; water treatment; general sanitation; crate washing;bottle soaking and washing; cap and bottle preparation; and as abeverage ingredient.

FIG. 5 schematically illustrates an improved bottled water processingand packaging system 6 which utilizes anolyte and catholyte treatmentsin accordance with the present invention. The improved bottled waterline 6 includes an electro-chemical activation system/reactor 8 forgenerating the anolyte and catholyte materials used. Examples ofsystems, subsystems and points within the bottled water line 6 whereinconcentrated catholyte or aqueous diluted catholyte washing solutionsare used include: the CIP system; bottle washing; and bottle washingcaustic bath and soaking operations. Examples of systems, subsystems andpoints wherein concentrated anolyte or aqueous diluted anolytedisinfecting wash solutions are used include: the CIP system; watertreatment; general sanitation; crate washing; bottle washing; causticbath applications; and finished product.

FIG. 6 illustrates an improved fruit juice production, processing, andbottling system 10 wherein ECWA solutions are used in accordance withthe present invention. The fruit juice line 10 includes anelectrochemical activation system/reactor 12 which produces anolyte andcatholyte materials used in the inventive process. Examples of systems,subsystems and points wherein concentrated catholyte or aqueous dilutedcatholyte wash solutions are used in the fruit juice line 10 include theCIP system, bottle washing, and mixing. Examples of systems, subsystemsand points wherein concentrated or aqueous diluted anolyte disinfectingsolutions are used in accordance with the inventive process include: theCIP system; general sanitation; crate washing; bottle washing; watertreatment; and as a product ingredient.

FIG. 7 schematically illustrates an improved wine production andbottling system 14 wherein ECAW is used in accordance with the presentinvention for several purposes. The improved wine production andbottling line 14 includes an electrochemical activation system/reactor16 for producing the anolyte and catholyte materials used in theimproved process. In the improved wine production and bottling line 14,examples of systems, subsystems, and points wherein concentratedcatholyte or aqueous diluted catholyte washing solutions are usedinclude the CIP system, bottle washing, manufacturing, and bottling.Examples of systems, subsystems and points wherein concentrated anolyteor aqueous diluted anolyte sanitizing solutions are used in the wineproduction and bottling line 14 include: the CIP system; watertreatment; general sanitation; crate washing; and bottle washing.

FIG. 8 schematically illustrates an improved beer production andbottling system 18 wherein ECAW is used in accordance with the presentinvention for various purposes. The improved beer production andbottling line 18 includes an electrochemical activation system/reactor20 for generating the anolyte and catholyte materials used in theimproved system. Examples of systems, subsystems and points whereinconcentrated catholyte or aqueous diluted catholyte wash solutions areemployed in the improved beer production and bottling line 18 includethe CIP system, bottle washing, manufacturing, and bottling. Examples ofsystems, subsystems and points wherein concentrated anolyte or aqueousdiluted anolyte disinfecting solutions are employed in the improved beerprocessing and bottling line 18 include: the CIP system; generalsanitation; water treatment; crate washing; bottle washing; and as abeer ingredient.

The inventive method also includes the use of electrochemicallyactivated aqueous anolyte as a disinfectant remedy against generalmicrobial and specific biofilm contamination of the charcoal granules ina GAC filtration system. The REDOX potential of the anolyte solution atvarious dilutions is employed to manipulate the surface charge and hencethe free energy of the charcoal granules, which supports the microbialand biofilm presence. This intervention comprises the step of contactingthe granular charcoal material with an anolyte solution having a pH(undiluted) in the range of from about 4.5 to about 7.5 and an ORP(undiluted) in the range of from about +650 mV to ≧+900 mV, preferablyby introducing the anolyte into the process water used in flushing theGAC system.

The invention further includes an electrochemically activated aqueousanolyte product with a pH (undiluted) in the range of from about 4.5 toabout 7.5 and an ORP (undiluted) in the range of from about +650 mV to≧+900 mV for use, preferably in aqueous diluted form, as a treatmentagent for the process water used in the disinfection of the systems andequipment used in the production, processing, and packaging of diversebeverage products.

The invention also extends to the use of electrochemically activatedaqueous anolyte as an oxidant in the elimination of contaminatingchemical residues, including dedicated product flavors and ingredientsencountered, for example, when switching a beverage system from theproduction of one beverage product to another. This step comprisescontacting the system and equipment components with an anolyte having apH (undiluted) in the range of from about 4.5 to about 7.5, an ORP(undiluted) in the range of from about +650 mV to ≧+900 mV and a FreeAvailable Oxidant concentration (undiluted) of <300 ppm. The anolyte ispreferably applied in aqueous diluted form.

The invention further includes an electrochemically activated aqueousanolyte with a pH (undiluted) in the range of from about 4.5 to about7.5, an ORP (undiluted) in the range of from about +650 mV to ≧+900 mV,and a Free Available Oxidant concentration (undiluted) of ≦300 ppm, foruse as an oxidant in the treatment of process water to eliminatepesticide and fungicide residues.

The invention also includes an electrochemically activated aqueousanolyte with a pH (undiluted) in the range of from about 4.5 to about7.5, an ORP (undiluted) in the range of from about +650 mV to ≧+900 mV,and a Free Available Oxidant concentration (undiluted) of ≦300 ppm, foruse as a treatment agent for the decontamination of the pore surfaces ofcarbon granules, as well as for the neutralization of pesticideresidues, in Granular Activated Charcoal columns.

The following is an example of a preferred procedure for the treatmentof granular activated charcoal (GAC) columns with electrochemicallyactivated water (ECAW) solutions. This procedure is described as relatedto standard filtration systems using GAC. The application protocol canbe readily adapted to accommodate differences in the design of thefiltration vessels and/or the flow dynamics of the filtrate.

The inventive process desirably uses the unique attributes of theenergized ECAW solutions to disrupt the surface free energy and thus theintrinsic charge environment of the GAC granules, and further uses thismanipulation of charge to effect a release of electrostatically boundbiofilm soils and organic debris from the charcoal surface, as well asto scavenge labile energy from the system as a dedicated biocidalintervention.

This is reliably and effectively achieved by the sequential applicationof ECAW catholyte and anolyte solutions. The mobilization and removal ofthe established organic soiling and biofilm growth by the introductionof the “energy-rich” catholyte solution is facilitated by thecatholyte's latent detergent and de-agglomerative reducing properties.Similarly, the neutralization of the free floating and granule-adherentmicrobes within the GAC bed is achieved by the presence of the highoxidant anolyte solution.

In terms of evaluating the performance of the two ECAW solutions, themeasurement of the physio-chemical properties of the solutions beforeand after delivery through the GAC vessel can be used to calculate thedegree of intervention achieved. However, it will be appreciated thatthe charge on the GAC granules will be altered in a progressive andcumulative manner, and that a gradient of altered charge through thedepth of the column will develop as a result of contact with the ECAWsolutions. Thus, the granules in contact with the ‘fresh’ solution atthe point of application will display the greatest alteration in chargewith the effect being progressively diluted as the ECAW solutionspercolate through the GAC bed. This charge ‘sacrifice’ is a result ofthe energy demand placed on the applied filtrate solution by the surfacefree energy of the granules, and requires either continuous flow orrepetitive applications of the ECAW solutions to progressively increasethe degree of charge alteration to the granules at increasing depthswithin the GAC column.

Thus, the less difference that is observed between the measuredproperties of the ECAW influent and effluent solutions, the greater thedegree of efficacy that will have been achieved. Catholyte solutionsshould thus be maintained effectively reducing throughout the GAC bedwhile the anolyte solutions should be maintained at a high oxidantstate.

For purposes of illustration, the procedure provided by the presentinvention is now described using the standard vessel design shown inFIG. 9.

In order to optimize the integrity of the physio-chemical measurementsused to predict the performance of the different ECAW solutions, thebaseline values of these same properties for the water stream in the GACcolumn prior to introducing any ECAW solutions are preferably firstmeasured. The same sets of measurements for both the influent andeffluent water stream are captured to determine the current performanceof the GAC granules in terms of influencing filtrate water quality, aswell as to serve as a base-line for comparison with the effects of theintervention with the ECAW solutions.

The data is interpreted in terms of the age of the granules in thecolumn and the current practices with regard to disinfection and chargeregeneration/rehabilitation, as well as the design and flow dynamics ofthe filtration vessel.

These measurements preferably comprise the following:

Oxidation reduction potential (ORP)— milliVolts (mV)Electrical Conductivity (EC)— milliSiemens/centimeter (mS/cm)Free Active Oxidants (FAO)— parts per million/milligram/liter(ppm/mg/lit)

Typically, the solutions used in the inventive GAC treatment willpreferably be of the following measured values and minimum volumes:

Solution ORP (mV) pH EC (mS/cm) Volume (lit) Anolyte ≧+900 ±6.5-7.0±5.5-6.0 3000 Catholyte ≦−900 ±11.0 ±5.5-6.0 3000The preferred procedure for treating the GAC column illustrated in FIG.9 with ECAW solutions is as follow:

-   -   1. Drain all possible residual water out of the GAC vessel.    -   2. Fresh solutions of Anolyte and Catholyte are preferably        generated on-site in sufficient quantities to permit a        continuous treatment to be undertaken.    -   3. Measure the ORP, pH and EC of the Catholyte at the inlet        treatment point of the vessel.    -   4. Fill the GAC vessel with concentrated Catholyte solution in a        normograde flow direction and allow the catholyte solution to        fill above the level of the carbon bed.    -   5. The Catholyte solution can be dosed in through the port at        the top of the vessel or through the existing inlet pipe which        connects to the upper distribution bellmouth. This will        typically require 5-20 minutes.    -   6. Allow the Catholyte solution to drain freely through the        bottom drain port or valve. This will typically take 5-10        minutes.    -   7. Measure the ORP, pH and EC of the effluent Catholyte solution        at the outlet point of the vessel.    -   8. Repeat the dosing of the Catholyte solution in a retrograde        flow direction (i.e. from the bottom upwards) after measuring        the ORP, pH and EC of the solution.    -   9. Allow the Catholyte solution to drain freely and measure the        ORP, pH and EC of the effluent solution.    -   10. Repeat the dosing and measurements as detailed in steps 8        and 9.    -   11. Repeat the normograde dosing of Catholyte in accordance with        the procedures detailed in steps 5-7.    -   12. While two repeated applications of the Catholyte solution        will typically be adequate to mobilize biofilm aggregations, the        number of repetitions of the dosing schedule may be increased,        and this will be governed by the degree of biofilm growth,        organic soiling or microbial bioload.    -   13. The vessel will preferably be drained completely of all        possible residual Catholyte effluent.

Anolyte Dosing

-   -   14. Measure the ORP, pH and EC of the Anolyte at the inlet        treatment point of the vessel.    -   15. Fill the GAC vessel with concentrated Anolyte solution in a        normograde flow direction and allow the Anolyte solution to fill        above the level of the carbon bed.    -   16. The Anolyte solution can be dosed in through the port at the        top of the vessel or through the existing inlet pipe which        connects to the upper distribution bellmouth. This will        typically take 5-20 minutes.    -   17. Allow the Anolyte solution to drain freely through the        bottom drain port or valve. This will typically take 5-10        minutes.    -   18. Measure the ORP, pH and EC of the effluent Anolyte solution        at the outlet point of the vessel.    -   19. Repeat the dosing of the Anolyte solution in a retrograde        flow direction (i.e. from the bottom upwards) after measuring        the ORP, pH and EC of the solution.    -   20. Allow Anolyte solution to drain freely and measure the ORP,        pH and EC of the effluent solution.    -   21. Repeat the dosing and measurements as detailed in steps 19        and 20.    -   22. Repeat the normograde dosing of Anolyte in accordance with        the procedures detailed in steps 16-18.    -   23. Drain all residual Anolyte effluent from the system and        introduce softened treated water to flush residual ECAW        solutions from the GAC filtration system. This will have been        accomplished when parity is achieved between the physio-chemical        properties of the influent water and the effluent water streams.

In addition to rehabilitating the charge of and to disinfecting theactivated carbon granules, the use of ECAW solutions used in accordancewith the inventive method further operates to neutralize pesticideresidues and build-up in the GAC system.

Without limiting the scope thereof, the invention will now be furtherdescribed and exemplified with reference to the following examples andexperimental results.

Example 1

This was a comparative test involving the use of ECAW solutions toreplace the existing chemical agents used in conventionalCleaning-in-Place (CIP) protocols. As shown below, the inventive methodprovided enhanced microbial control, reduced water usage, and shortercleaning and disinfection cycles in a carbonated beverage plant.

Conventional cleaning and disinfection of systems and equipment incarbonated beverage packaging plants has typically comprised twoprotocols—either a three step (only disinfection) or a five step process(cleaning, rinsing and disinfection).

Antioxidant catholyte and oxidant anolyte were added to process waterused for the cleaning and disinfection of production and packagingsystems and equipment for diverse beverage types as a completesubstitution for existing conventional chemical products. The measuredcharacteristics of the diluted aqueous treatment solutions used were asfollows:

Solution* EC** pH ORP FAO  5% Anolyte 0.67 6.6 740 <25 30% Catholyte2.72 10.8 220 0 30% Anolyte 2.0 6.8 890 80 *Solution concentrationsexpressed as vol %. **Electrical conductivity (mS/cm—milliSiemens percentimeter)

A comparative trial was conducted in a representative carbonatedbeverage manufacturing and packaging plant. The conventional cleaningchemicals used in the comparative trial comprised a 2-3% chlor-alkalinecaustic soda (NaOH) solution employed at ambient temperature. Theconventional disinfectant solution comprised either a sodium or calciumhypochlorite solution or equivalent oxidant agent dosed at ambienttemperature into the system at a rate of 50 ppm of Free AvailableChlorine (FAC) content. The protocols for the conventional procedurewere as follows:

TABLE 1 CIP protocols using conventional chemicals Process Step 5 Step 3Step Initial Rinse with treated 5 to 10 minutes 5 to 10 minutes water±7000 l treated water used ±7000 l treated water used Detergent Cleaning15 to 20 minutes @ 2.5% chloralkali Excludes time for manual CIP ±10000l treated water used changeover - Est. 20 minutes Treated water rinse 5to 10 minutes 5 to 10 minutes ±7000 l treated water used ±7000 l treatedwater used Sanitation 20 to 30 minutes @ 50 mg/l 20 minutes @ 50 mg/l±10000 l treated water used ±10000 l treated water used Treated waterRinse 5 to 10 minutes 5 to 10 minutes ±7000 l treated water used ±7000 ltreated water used TOTAL TIME 50-80 minutes 35 to 50 minutes TotalSolution Usage ±41,000 l CIP solution used ±31,000 l treated water used

For purposes of comparison, the following protocols were then initiatedusing the ECAW solutions in accordance with the inventive method:

TABLE 2 CIP protocols using the ECA solutions Process Step 5 Step 3 StepInitial Rinse with 5% Anolyte <10 minutes <10 minutes treated water±3000 l treated water used ±3000 l treated water used Detergent Cleaning15 minutes @ 30% Catholyte Nil ±3000 l treated water used Treated waterrinse Nil Nil Sanitation 15 minutes @ 30% Anolyte 15 minutes @ 30%Anolyte ±3000 l treated water used ±3000 l treated water used Treatedwater Rinse <10 minutes <10 minutes ±3000 l treated water used ±3000 ltreated water used TOTAL TIME 50 minutes 35 minutes Total Solution Usage±12,000 l CIP solution used ±9,000 l treated water used

The antimicrobial efficacy of the oxidant anolyte solution is reflectedin FIGS. 1, 2 & 3.

A standard membrane filtration method was used to test allmicrobiological samples. Swabs were collected as per recognized standardprotocols.

Conclusions:

Aside from the complete elimination of conventional cleaning anddisinfecting chemicals, the integration of the ECA solutions into boththe 3 and 5 step CIP procedures resulted in a significant reduction inwater usage and a substantial saving in the time required to completethe CIP process.

Example 2 Carbonation of ECA Solutions

Carbonation of predetermined, diluted ECA solutions was conducted toestablish the changes in the physiochemical characteristics thatresulted from the addition and presence of gaseous Carbon Dioxide (CO₂).

Standard dilutions of freshly generated ECA anolyte and catholyte wereprepared using untreated potable process water. The physiochemicalattributes of each solution were recorded both before and aftercarbonation in order to detail the changes effected by the introductionof CO₂.

As will be understood by those in the art, the various solutions testedin this example were carbonated by the application of 2.5 volumes (5gm/500 ml) of CO₂ to 500 ml of the sample at ambient temperature for 30seconds.

TABLE 3 Physiochemical parameters of the ECA solutions before and aftercarbonation. Catholyte @ 30% Concentrate Parameter Before AfterCatholyte EC (mS) 3.38 2.53 9.93 pH 11.3 5.4 11.6 ORP (mV) 15 441 −110Anolyte @ 30% Concentrate Parameter Before After Anolyte EC (mS) 2.82.63 8.14 pH 6.9 4.7 7.0 ORP (mV) 830 980 885 FAO (ppm) 80 80 +200Anolyte @ 5% Parameter Before After EC (mS) 0.69 0.6 pH 6.9 4.7 ORP (mV)823 930 FAO (ppm) 20-25 20-25 Legend: ORP—Oxidation-Reduction Potential(mV—milliVolt), EC—Electrical Conductivity - (mS/cm—milliSiemens percentimeter), FAO—Free Available Oxidants (ppm—parts per million)

In terms of the Catholyte solution, there was a substantial shift inREDOX potential from a substantially reducing capability to being a weakoxidant.

It has been repeatedly demonstrated that ORP is a reliable measure ofpotential antimicrobial efficacy of anolyte solutions at differentdilution rates and that, with a prior knowledge of the extent ofmicrobial bioload (cfu/ml) in a system, the anolyte solution required toeliminate microbial contamination can be accurately titrated on thebasis of this relationship. The addition of CO₂ to the diluted anolytesolutions resulted in a surprising and substantial upwards shift inREDOX potential with an increased oxidant activity and was paralleled byan equivalent reduction in pH which also serves to potentiate thebiocidal activity of the ECA disinfectant solutions.

Conclusion:

The carbonation of ECA solutions results in substantial shifts in thephysicochemical parameters affecting cleaning and microbicidal capacity.The elevated REDOX potential of the carbonated anolyte provides anenhanced antimicrobial capability relative to non-carbonated anolyte.

Example 3 Residue Neutralization

The breakdown of pesticide and fungicide residues by an oxidant ECAanolyte solution was evaluated as follows.

The oxidant anolyte solution was diluted using a 10 fold dilutionseries. As a control for this test, the potential for non-ECA basedhydrolysis or chemical breakdown was assessed using two untreatedcontrol solutions, one being the tap water used as the diluent in theanolyte dilution series and the other being the non-activated brinesolution that was used as the electrolysis feed solution prior toelectro-activation.

The experiment was performed to contrast the difference in degree ofrecovery of a variety of pesticide and fungicide active ingredients(AI's) after the tap water and the various diluted anolyte solutionswere ‘spiked’ with the same AI's at fixed inclusion rates. In each case,a one ppm cocktail of the active ingredients was added to a 100 mlaliquot of the test or control solution sample. The test samples wereagitated with a mechanical stirrer for 5 minutes at ambient temperatureand then extracted with an organic solvent and analyzed by either gas orliquid chromatography.

TABLE 4 Physiochemical parameters of the control and anolyte testsolutions Solution type ORP (mV) pH EC (mS/cm) FAO (ppm) Tap watercontrol 280 8.2 0.21 — 2.5 gm/lit salt solution 290 7.7 5.22 —nonactivated  1% Anolyte solution 436 7.5 0.35  ≦5  10% Anolyte solution803 7.2 1.34 20-25 100% Anolyte solution 940 6.5 5.45 ≦200 Legend:ORP—Oxidation-Reduction Potential (mV—milliVolts), EC—ElectricalConductivity (mS/cm—milliSiemens per centimeter), FAO—Free AvailableOxidant concentration (ppm—parts per million).

TABLE 5 Mass and percentage recovery and breakdown of a range ofpesticide and fungicide Active Ingredients (AI's) after exposure to avariety of anolyte dilutions. 0.25% Brine 1% Anolyte solution 10%anolyte solution 100% anolyte solution Tap % % % % Active water ngrecov- ng % break- ng % break- ng % break- Ingredient Chemical type (ng)found ery found recovery down found recovery down found recovery downMalathion Organophosphorus 0.066 1,327 126.1 1.368 130.2 0.0 0.066 0.0100 0.067 0.1 100 insecticide Chlorpyrifos Organophosphorus 0.05 1.01496.4 1.039 98.9 0.0 0.05 0.0 100 0.049 −0.1 100 insecticide CyprodinilAnilino-pyrimidine 0.031 1.297 126.6 1.356 132.5 0.0 0.068 3.7 96.30.026 −0.5 100 fungicide Kresoxim- Strobilurin 0.029 1.300 127.1 1.328129.9 0.0 1.344 131.5 0.0 0.035 0.6 100 methyl fungicide BupirimatePyrimidine 0.052 1.250 119.8 1.233 118.1 0.0 0.730 67.8 52.0 0.074 2.2100 Fungicide Azinphos- Organophosphorus 0.095 2.341 224.6 2.393 229.80.0 0.000 −9.5 100 0.000 −9.5 100 methyl insecticide BenomylBenzimadazole 0.000 0.970 97.0 0.890 89.0 8.0 0.520 52.0 45 0.000 0.0100 fungicide Aldicarb Carbamate 0.000 0.920 92.0 0.425 42.5 49.5 0.0000.0 100 0.000 0.0 100 insecticide Aldicarb Carbamate 0.000 0.672 67.20.514 51.4 15.8 0.000 0.0 100 0.000 0.0 100 sulfoxide insecticideMethomyl Carbamate 0.000 1.006 100.6 0.634 63.4 36.6 0.000 0.0 100 0.0000.0 100 insecticide Legend: ng—nanograms

CONCLUSION

The organophosphorus and carbamate group pesticides and thebenzimidazole, anilinopyrimidine, strobilurin, pyrimidine, andbenzimidazole based fungicides were all oxidized by exposure to theanolyte solutions.

Example 4 Microbial Decontamination and Surface Free Energy Manipulationof Activated Charcoal Granules with ECA Solutions

ECA solutions were applied to a standard Granular Activated Charcoal(GAC) column vessel with an active filtration bed dimension of 2000 mmdepth and 1700 mm diameter. Commercial (F200 grade) activated charcoalgranules with a bulk density of 500 kg/m³ were overlaid above with agraduated pebble bed of varying sizes and densities. The charcoalgranule bed had become progressively contaminated with a maturemicrobial biofilm and optimal operational rehabilitation of the granulesusing conventional procedures would have required either extended steampasteurization or complete replacement of the granules.

In light of the specific adsorption characteristics of the charcoalgranules based on surface free energy, an antioxidant catholyte wasinitially used to manipulate the surface tension of the filtrate waterat the biofilm:charcoal granule interface promoting the disruption ofthe adsorbed inorganic biofilm matrix. The changes in the physiochemicalattributes of the influent solutions were contrasted against those ofthe effluent stream and these differences described the degree ofsurface free energy manipulation achieved as well as served to predictthe degree of alteration of adsorptive capacity at the charcoal granulesurface.

Following continuous catholyte infusion, steeping and drainage, ananolyte solution was introduced and the physiochemical characteristicsof both the influent and effluent streams were contrasted to detail whenthe optimum Oxidation Reduction Potential had been attained within thebed in order to achieve the required antimicrobial effect.

Optimal admixture of the ECA solutions with the surfaces of the charcoalgranules was achieved by introducing the ECA solutions from both the topas well as the bottom of the filter vessel and this protocol increasedgranule surface exposure by disrupting the channeling of filtratethrough existing flow configurations in the granule bed.

TABLE 6 Changes in the physiochemical attributes of the ECA solutionsapplied to a GAC vessel over time Changes in physiochemical parametersof Catholyte and Anolyte solutions when introduced into a GranularActivated Charcoal column over time Δ ORP Feed- Time Solution typeActivity ORP pH EC Effluent Anolyte Pretreatment 935 6.6 5.15 CatholytePretreatment −804 11.1 6.61 09:10 Catholyte Pump Top −804 11.1 6.6109:20 Catholyte drain 65 9.8 5.15 −869 09:26 Catholyte 85 9.9 4.77 −88909:43 Catholyte pump bottom −804 11.1 6.61 10:21 Catholyte drain 5 11.16.35 −809 10:23 Catholyte 18 11.1 6 −822 10:24 Catholyte pump bottom−804 11.1 6.61 10:42 Catholyte drain 50 11.1 6 −854 10:45 Catholyte pumptop + drain −804 11.1 6.61 10:48 Catholyte drain 9 11.2 6.39 −813 10:52Catholyte −3 11.3 6.32 −801 11:00 Catholyte 32 11.1 5.51 −836 11:07Catholyte 35 10.7 5.03 −839 11:12 Catholyte 54 10 5.29 −858 11:15Catholyte 184 9.7 4.18 −988 11:20 Anolyte pump top + drain 935 6.6 5.1511:22 Anolyte drain 295 9.9 4.98 640 11:28 Anolyte 274 9.7 5.26 66111:38 Anolyte 334 9.2 5.26 601 11:47 Anolyte 256 9.5 5.26 679 11:49Anolyte pump top, no drain 935 6.6 5.15 12:15 Anolyte drain 215 9 5.21720 12:21 Anolyte 245 9 4.93 690 12:30 Anolyte pump bottom 935 6.6 5.1513:06 Anolyte Pump top 935 6.6 5.15 13:20 Anolyte 844 7.4 5.19 91 13:23Anolyte 792 7.5 5.15 143 13:28 Anolyte 391 8.6 5.2 544 13:35 Anolytepump bottom 935 6.6 5.15 14:06 Anolyte Pump top 935 6.6 5.15 14:18Anolyte drain 843 7.5 5.27 92 14:22 Anolyte steep 831 7.4 5.24 104Legend: ORP—Oxidation Reduction Potential (mV—milliVolts), EC—ElectricalConductivity (mS/cm—milliSiemens per centimeter)

CONCLUSION

It was demonstrated that the elevated Oxidation Reduction Potential(ORP) of the electrochemically activated Catholyte and Anolytesolutions, when applied as a tandem and sequential intervention toGranular Activated Charcoal (GAC) filtration columns, has the capacityto selectively manipulate the surface free energy charge on the surfacesand within the pores of the charcoal granules used for filtration andadsorption in beverage processing and packaging plants, as well as inother applications. This capacity serves to assist in the regenerationof the absorption characteristics of the granules as well as tosubstantially reduce the microbial burden both on the surfaces as wellas within the pores of the granules.

Example 5 Flavor Neutralization Capacity of ECA Solutions

It has further been discovered in accordance with the present inventionthat anolyte solutions can surprisingly provide an added benefit inthat, in addition to its broad based antimicrobial efficacy, anolyte isable simultaneously to oxidize residual flavorant molecules andsynthetic ingredient residues from manufacturing and packagingequipment.

The trial involved an organoleptic and calorimetric appraisal of thecapacity of ECA solutions to eliminate persistent and robust flavorfingerprints from packaging equipment in a carbonated beverage plant.

The change from one particularly persistent and robust flavor type(pineapple based) to a standard cola flavor or soda water based product,demonstrated a complete elimination of residual carry-over of theflavorant substance after exposure to the ECA solutions.

Additionally, in-vitro testing with a range of commercial syntheticflavor molecules (Cranbrook Flavors) including Apple (MJ3116), Chemy(MJ2381), Raspberry (MJ3102), Blackcurrent (MJ1115), Pineapple (MJ2082),Bubblegum (MG1250) and Strawberry (MJ2507) all demonstrated effectiveneutralization in the ECA solutions spiked with the flavor molecules.

Conclusion: ECA anolyte solutions have the ability to neutralizepersistent and robust flavor molecules.

Example 6

An ECAW anolyte product was continuously dosed into well water used forbeer production. During the course of the trial, the concentratedanolyte used in the test was maintained at a pH of about 6.5±0.5, an ORP(millivolts) of 900±50, and an electrical conductivity (mSiemens/cm) of5.5±0.5. The resulting treated well water had an anolyte concentrationof 0.5% by volume, a pH of 6.5±0.5, an ORP of 500±50, and an electricalconductivity of 0.2±0.05.

After steady state conditions were achieved, the treated well water wasrendered microbe free. The treated well water was used as an actualingredient for beer production. No adverse effects from the use of thetreated water were detected in the taste, character, color or othercharacteristics of the beer product.

Thus, the present invention is well adapted to carry out the objectivesand attain the ends and advantages mentioned above as well as thoseinherent therein. While presently preferred embodiments have beendescribed for purposes of this disclosure, numerous changes andmodifications will be apparent to those of ordinary skill in the art.Such changes and modifications are encompassed within this invention asdefined by the claims.

1. A method of rehabilitating and disinfecting a granular activatedcharcoal bed used for purifying water comprising the non-simultaneoussteps of: (a) contacting said granular activated charcoal bed with anelectrochemically-activated water catholyte solution and (b) contactingsaid granular activated charcoal bed with an electrochemically-activatedwater anolyte solution.
 2. The method of claim 1 wherein: when inundiluted form, said electrochemically-activated water catholytesolution has a negative oxidation-reduction potential of at least −110mV and a pH in a range of from about 8 to about 13 and when in undilutedform, said electrochemically-activated water anolyte solution has apositive oxidation-reduction potential of at least +650 mV and a pH in arange of from about 4.5 to about 7.5.
 3. The method of claim 2 whereinsaid negative oxidation-reduction potential of saidelectrochemically-activated water catholyte solution is at least ˜700mV.
 4. The method of claim 2 wherein: said electrochemically-activatedwater catholyte solution is used in undiluted form for contacting saidgranular activated charcoal bed in step (a) and saidelectrochemically-activated water anolyte solution is used in undilutedform for contacting said granular activated charcoal bed in step (b). 5.The method of claim 1 wherein: said electrochemically-activated wateranolyte solution has a beginning oxidation-reduction potential prior tocontacting said granular activated charcoal bed; said beginningoxidation-reduction potential is a positive mV oxidizing value; saidelectrochemically-activated water anolyte solution has a spentoxidation-reduction potential after being used for contacting saidgranular activated charcoal bed; and step (b) comprises the steps of:(i) determining said beginning oxidation-reduction potential of saidelectrochemically-activated water anolyte solution, (ii) contacting saidgranular activated charcoal bed with said electrochemically-activatedwater anolyte solution, (iii) determining said spent oxidation-reductionpotential of said electrochemically-activated water anolyte solutionafter step (ii) and (iv) repeating steps (ii) and (iii) at least untilsaid spent oxidation-reduction potential of saidelectrochemically-activated water anolyte solution determined in step(iii) is a positive mV oxidizing value which is not more than 544 mVless than said beginning oxidation-reduction potential of saidelectrochemically-activated water anolyte solution.
 6. The method ofclaim 5 wherein said beginning oxidation-reduction potential of saidelectrochemically-activated water anolyte solution is at least +650 mV.7. The method of claim 5 wherein, in step (iv), steps (ii) and (iii) arerepeated at least until said spent oxidation-reduction potential of saidelectrochemically-activated water anolyte solution determined in step(iii) is not more than 143 mV less than said beginningoxidation-reduction potential of said electrochemically-activated wateranolyte solution.
 8. The method of claim 5 wherein, in step (iv), steps(ii) and (iii) are repeated at least until said spentoxidation-reduction potential of said electrochemically-activated wateranolyte solution determined in step (iii) is not more than 104 mV lessthan said beginning oxidation-reduction potential of saidelectrochemically-activated water anolyte solution.
 9. The method ofclaim 1 wherein step (b) is conducted at least twice such that: saidelectrochemically-activated water anolyte solution is at least oncedelivered to said granular activated charcoal bed in a substantiallynormal operating flow direction and said electrochemically-activatedwater anolyte solution is at least once delivered to said granularactivated charcoal bed in a reverse flow direction which issubstantially opposite said substantially normal operating flowdirection.
 10. The method of claim 1 wherein step (a) is conducted atleast twice such that: said electrochemically-activated water catholytesolution is at least once delivered to said granular activated charcoalbed in a substantially normal operating flow direction and saidelectrochemically-activated water catholyte solution is at least oncedelivered to said granular activated charcoal bed in a reverse flowdirection which is substantially opposite said substantially normaloperating flow direction.